CN108732387A - A kind of probe sample distance controlling method and system of SICM - Google Patents
A kind of probe sample distance controlling method and system of SICM Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及扫描离子电导显微镜(SICM)成像技术领域,特别涉及一种SICM成像时其探针与样品间距的自适应控制方法及系统。The invention relates to the technical field of scanning ion conductance microscope (SICM) imaging, in particular to an adaptive control method and system for the distance between a probe and a sample during SICM imaging.
背景技术Background technique
扫描离子电导显微镜(scanning ion conductance microscope:SICM)是一种在生物、医药、化学、材料等领域均得到广泛应用的扫描探针显微镜,与传统光学显微镜相比具有分辨率更高的特点,光学显微镜受光学衍射极限的限制分辨率无法达到200nm以下,而扫描探针显微镜以其探针与样品表面的相互作用作为成像依据,不受光学衍射极限的影响,分辨率可达几纳米或几十纳米;SICM与其他扫描探针显微镜相比,其特点在于能够在生理条件下对活细胞进行非力接触的无损观测,同时不需要对样品进行荧光标记等预处理,因而是一种高分辨率、高保真的成像技术,特别适用于对柔软样品如活细胞等的观测。SICM采用一根尖端为锥形、尖端内半径约为几十到几百纳米的超微中空玻璃管作为探针,待测样品放置在灌有电解质溶液的样品皿中,探针中也灌有相同的溶液,并且在样品皿和探针中各置有一根AgCl电极,在电极两端施加电压,就会与电解质溶液共同构成电流回路,产生离子电流。当针尖与样品表面距离较远时,离子电流保持在一个恒定值,当探针距离样品足够近,针尖与样品间狭小的缝隙就会阻碍离子的流过,使离子电流减小,离子电流与探针样品的间距存在一一对应的曲线关系,因而可以用电流来表征探针与样品表面的距离。在对样品进行成像时,使探针在样品表面逐行扫过,实时监控电流的大小,通过负反馈控制探针在垂直方向的移动使离子电流维持在一个固定的值,相当于探针在样品表面保持一个恒定的高度,于是记录下探针移动的轨迹即可得到样品表面的三维形貌。Scanning ion conductance microscope (SICM) is a scanning probe microscope widely used in biology, medicine, chemistry, materials and other fields. Compared with traditional optical microscope, it has higher resolution. The microscope is limited by the optical diffraction limit, and the resolution cannot reach below 200nm, while the scanning probe microscope uses the interaction between its probe and the sample surface as the imaging basis, and is not affected by the optical diffraction limit, and the resolution can reach several nanometers or tens of nanometers. Nano; Compared with other scanning probe microscopes, SICM is characterized by the non-destructive observation of living cells under physiological conditions without force contact, and does not require pretreatment of samples such as fluorescent labeling, so it is a high-resolution, High-fidelity imaging technology is especially suitable for the observation of soft samples such as living cells. SICM uses an ultra-micro hollow glass tube with a tapered tip and an inner radius of tens to hundreds of nanometers as a probe. The sample to be tested is placed in a sample dish filled with electrolyte solution, and the probe is also filled with The same solution, and an AgCl electrode is placed in the sample vessel and the probe, and a voltage is applied to both ends of the electrode to form a current loop together with the electrolyte solution to generate an ionic current. When the distance between the needle tip and the sample surface is far away, the ion current remains at a constant value. When the probe is close enough to the sample, the narrow gap between the needle tip and the sample will hinder the flow of ions and reduce the ion current. There is a one-to-one curve relationship between the distance between the probe and the sample, so the current can be used to characterize the distance between the probe and the sample surface. When imaging the sample, the probe is scanned across the surface of the sample line by line, the magnitude of the current is monitored in real time, and the movement of the probe in the vertical direction is controlled by negative feedback to maintain the ion current at a fixed value, which is equivalent to the probe in the The sample surface maintains a constant height, so the three-dimensional shape of the sample surface can be obtained by recording the trajectory of the probe movement.
现有的SICM探针样品距离控制的方式为普通PID控制,在使用SICM对样品进行的大量成像实验中发现,SICM所成图像存在拖尾现象,表现为当采用某一PID参数时,在样品高度的上升沿处展现了样品的真实形貌,而在高度的下降沿处图像形貌比实际形貌有一定的延长,即在上升沿探针及时的跟踪到了高度的变化,而在下降沿探针跟踪样品高度变化的速度较慢。这一现象影响了SICM对样品形貌的真实反映,使得扫描图像与真实形貌存在一定的偏差。通过分析发现,拖尾现象是由电流逼近曲线的非线性引起的,逼近曲线是探针逐渐逼近样品过程中离子电流变化的曲线,扫描时以逼近曲线中最大值的95%到99%作为设定值,使电流维持在设定值不变。由于逼近曲线的非线性,对于同样的高度变化下,在样品高度的上升沿,作为反馈量的电流偏差较大,而在下降沿,电流偏差较小,此时若采用相同的PID参数就会产生不同的控制量,使得探针跟踪的速度不同,在上升沿能够快速跟踪到样品高度的变化,而在下降沿需要更长的时间才能完成对高度的跟踪,产生了拖尾现象。The existing SICM probe sample distance control method is ordinary PID control. In a large number of imaging experiments using SICM on samples, it was found that the image formed by SICM has a tailing phenomenon, which is manifested as when a certain PID parameter is used. The rising edge of the height shows the real shape of the sample, and the image shape is longer than the actual shape at the falling edge of the height, that is, the probe tracks the height change in time on the rising edge, and the image shape on the falling edge Probes are slow to track changes in sample height. This phenomenon affects the real reflection of the sample morphology by SICM, which makes the scanning image deviate from the real morphology to a certain extent. Through analysis, it is found that the tailing phenomenon is caused by the nonlinearity of the current approximation curve. The approximation curve is the curve of ion current changes during the process of the probe gradually approaching the sample. When scanning, the maximum value in the approximation curve is set at 95% to 99%. fixed value to keep the current constant at the set value. Due to the non-linearity of the approximation curve, for the same height change, the current deviation as the feedback value is relatively large at the rising edge of the sample height, and the current deviation is small at the falling edge. If the same PID parameters are used at this time, the Different control values are generated, so that the speed of the probe tracking is different. The change of the sample height can be quickly tracked on the rising edge, but it takes longer to complete the tracking of the height on the falling edge, resulting in a tailing phenomenon.
发明内容Contents of the invention
为了解决上述由逼近曲线非线性所引起的SICM成像的下降沿拖尾现问题,本发明提供了一种探针/样品间距的自适应控制方法及系统。In order to solve the problem of trailing edge trailing in SICM imaging caused by the nonlinearity of the approximation curve, the present invention provides an adaptive control method and system for the probe/sample distance.
本发明采用的技术方案如下:一种SICM的探针与样品间距离自适应控制方法,包括以下步骤:The technical scheme adopted in the present invention is as follows: a method for self-adaptive control of the distance between a probe and a sample of SICM, comprising the following steps:
步骤1、扫描前建立逼近曲线,该逼近曲线为探针和样品间距离与离子电流的关系曲线;利用逼近曲线建立下降沿补偿函数模型,该模型以探针当前位置与工作点位置的Z轴压电陶瓷电压差值为输入,以下降沿补偿系数为输出;Step 1. Establish an approximation curve before scanning. The approximation curve is the relationship curve between the distance between the probe and the sample and the ion current; use the approximation curve to establish a falling edge compensation function model. The model is based on the Z axis between the current position of the probe and the position of the working point The piezoelectric ceramic voltage difference is the input, and the falling edge compensation coefficient is the output;
步骤2、扫描过程中将图像上一行的扫描高度作为当前待扫描行的工作点位置;Step 2. During the scanning process, the scanning height of the previous line of the image is used as the working point position of the current line to be scanned;
步骤3、扫描当前行时,采集压电陶瓷的实时位置,将探针当前位置与预测的工作点位置的Z轴压电陶瓷电压差值代入下降沿补偿函数,得到下降沿补偿系数;Step 3. When scanning the current line, collect the real-time position of the piezoelectric ceramic, and substitute the Z-axis piezoelectric ceramic voltage difference between the current position of the probe and the predicted working point position into the falling edge compensation function to obtain the falling edge compensation coefficient;
步骤4、判断当前位置是否为高度下降沿;若是则将离子电流偏差的比乘以下降沿补偿系数反馈至控制器;Step 4. Determine whether the current position is a height falling edge; if so, multiply the ratio of the ion current deviation by the falling edge compensation coefficient and feed it back to the controller;
步骤5、控制器输出控制量给压电陶瓷,使探针跟踪样品的形貌高度,与样品表面保持恒定的距离。Step 5, the controller outputs the control amount to the piezoelectric ceramics, so that the probe tracks the shape height of the sample and keeps a constant distance from the surface of the sample.
所述利用逼近曲线建立下降沿补偿函数模型具体为:利用逼近曲线通过拟合的方式建立下降沿补偿函数,该函数的输出为下降沿的电流偏差需要增加的倍数。The establishment of the falling edge compensation function model by using the approximation curve is specifically: using the approximation curve to establish the falling edge compensation function by fitting, and the output of the function is the multiple that the current deviation of the falling edge needs to increase.
所述利用逼近曲线建立下降沿补偿函数模型包括以下步骤:The establishment of the falling edge compensation function model using the approximation curve includes the following steps:
步骤1-2-1、以图像扫描时的电流设定值为中间点,将逼近曲线分成左、右即高度上升和高度下降两部分;Step 1-2-1. Taking the current setting value during image scanning as the middle point, divide the approximation curve into two parts: left and right, that is, height rise and height fall;
步骤1-2-2、在高度上升和高度下降两部分中,以离子电流与电流设定值之间的电流偏差的绝对值为函数值,以Z轴压电陶瓷电压与电流设定值处所对应的Z轴压电陶瓷电压之差的绝对值为自变量,用来表示探针当前位置到工作点位置的距离,分别做出上升沿和下降沿的电流偏差随Z轴压电陶瓷电压差值的变化曲线;上升沿的电流偏差为正偏差,下降沿的电流偏差负偏差;Step 1-2-2. In the two parts of height rise and height fall, the absolute value of the current deviation between the ion current and the current setting value is used as the function value, and the Z-axis piezoelectric ceramic voltage and current setting value are used. The absolute value of the corresponding Z-axis piezoelectric ceramic voltage difference is an independent variable, which is used to represent the distance from the current position of the probe to the working point. The change curve of the value; the current deviation of the rising edge is a positive deviation, and the current deviation of the falling edge is a negative deviation;
步骤1-2-3、以正偏差与负偏差绝对值的比作为函数值,以反映探针当前位置到工作点位置距离的Z轴压电陶瓷电压差值为自变量,采用最小二乘法进行有理数拟合得到系数,建立下降沿补偿函数。Step 1-2-3, using the ratio of the absolute value of the positive deviation to the negative deviation as the function value, taking the Z-axis piezoelectric ceramic voltage difference reflecting the distance from the current position of the probe to the working point as the independent variable, and using the least square method Coefficients are obtained by rational number fitting, and a falling edge compensation function is established.
所述下降沿补偿函数模型The falling edge compensation function models the
k(d)=(p1×d+p2)/(d+q1)k(d)=(p1×d+p2)/(d+q1)
其中k(d)为下降沿补偿系数,d为反映探针当前位置与工作点位置距离的Z轴压电陶瓷电压差值,p1,p2,q1为系数。Among them, k(d) is the falling edge compensation coefficient, d is the Z-axis piezoelectric ceramic voltage difference reflecting the distance between the current position of the probe and the working point, and p1, p2, q1 are coefficients.
所述步骤4包括以下步骤:Described step 4 comprises the following steps:
步骤4-1、实时采集离子电流及压电陶瓷电压;Step 4-1, collecting ion current and piezoelectric ceramic voltage in real time;
步骤4-2、判断当前扫描点是样品高度的上升沿还是下降沿;Step 4-2, judging whether the current scanning point is the rising edge or the falling edge of the sample height;
步骤4-3、如果是上升沿则电流偏差保持原来的值不变;否则更新电流偏差为原电流偏差、再乘以下降沿补偿系数k后反馈至控制器。Step 4-3. If it is a rising edge, the current deviation keeps the original value; otherwise, the current deviation is updated to the original current deviation, multiplied by the falling edge compensation coefficient k, and then fed back to the controller.
所述步骤4-2包括:Said step 4-2 comprises:
步骤4-2-1、分别设定一个离子电流偏差值、一个压电陶瓷的电压差值,作为死区;Step 4-2-1, respectively setting an ion current deviation value and a piezoelectric ceramic voltage difference value as the dead zone;
步骤4-2-2、当电流偏差和均超出死区时,判断为样品高度的下降沿,否则为高度上升沿。Step 4-2-2. When the sum of the current deviations exceeds the dead zone, it is judged as the falling edge of the sample height, otherwise it is judged as the rising edge of the height.
一种SICM探针与样品间距离的自适应控制系统,包括:An adaptive control system for the distance between a SICM probe and a sample, comprising:
逼近曲线模块:设定探针逼近停止点,获得逼近曲线数据;Approach curve module: set the probe approach stop point, and obtain the approach curve data;
下降沿补偿函数模型建立模块:设定扫描工作点,以工作点为中点通过逼近曲线绘制电流偏差随探针到工作点位置的距离变化的曲线,拟合得到正负偏差比值和反映探针当前位置到工作点位置距离的Z轴压电陶瓷电压差值的关系曲线,建立下降沿补偿函数模型;Falling edge compensation function model building module: set the scanning working point, use the working point as the midpoint to draw the curve of the current deviation with the distance from the probe to the working point through the approximation curve, and get the positive and negative deviation ratio and reflect the probe The relationship curve of the Z-axis piezoelectric ceramic voltage difference between the current position and the working point position, and the establishment of the falling edge compensation function model;
行预测模块:保存当前行每一点的高度信息,在对下一行扫描时提供给控制模块作为高度的预测值;Row prediction module: save the height information of each point in the current row, and provide it to the control module as the predicted value of height when scanning the next row;
反馈控制模块:用下降沿补偿函数模型处理电流偏差得到新的偏差,将新的偏差输入到PID控制器得到控制量,输出控制量到压电陶瓷控制探针的高度以跟踪样品表面的形貌。Feedback control module: Use the falling edge compensation function model to process the current deviation to obtain a new deviation, input the new deviation to the PID controller to obtain the control value, and output the control value to the piezoelectric ceramic to control the height of the probe to track the shape of the sample surface .
本发明具有如下优点:The present invention has the following advantages:
1、本发明可以消除SICM成像中的下降沿模糊现象。由于逼近曲线的非线性,使样品高度的上升沿和下降沿在同样的距离偏差下产生不同的电流偏差,进而导致控制量不同,使在下降沿探针跟踪形貌的速度较慢,产生了下降沿的模糊现象。本发明增加了下降沿处的电流偏差,使其与对应相同距离的上升沿处的电流偏差大小相同,解决了样品高度上升与下降沿的电流偏差差异,使下降沿获得了同样的探针跟踪速度,当设定某一PID参数使上升沿成像清晰时,下降沿也同样清晰。1. The present invention can eliminate the falling edge blur phenomenon in SICM imaging. Due to the nonlinearity of the approximation curve, the rising edge and falling edge of the sample height produce different current deviations under the same distance deviation, which leads to different control quantities, making the speed of the probe tracking the shape slower on the falling edge, resulting in Blurring of the falling edge. The present invention increases the current deviation at the falling edge, making it the same size as the current deviation at the rising edge corresponding to the same distance, and solves the current deviation difference between the rising and falling edges of the sample height, so that the falling edge can obtain the same probe tracking Speed, when a certain PID parameter is set to make the image of the rising edge clear, the falling edge is also clear.
2、本发明可以避免因PID参数过大而造成的振荡。使用原有的控制方法及系统,在扫描过程中当发现样品的高度下降沿处存在普遍的模糊时,会估计是由于探针跟踪速度过慢而造成的成像模糊,这是就会增大PID参数以加快探针对偏差的响应速度,而同时在上升沿处就会产生更大的控制量,增加超调和振荡的可能,不利于得到真实的形貌,甚至会损坏样品。使用了本发明后,上升沿和下降沿对应相同距离偏差输出的控制量相同,避免了上述情况的发生,更容易得到真实的形貌,同时对样品和仪器都有积极的保护作用。2. The present invention can avoid oscillation caused by excessive PID parameters. Using the original control method and system, when it is found that there is general ambiguity at the falling edge of the sample during the scanning process, it will be estimated that the imaging ambiguity is caused by the slow probe tracking speed, which will increase the PID parameters to speed up the response speed of the probe to the deviation, and at the same time, a greater amount of control will be generated at the rising edge, which increases the possibility of overshoot and oscillation, which is not conducive to obtaining the real shape, and even damages the sample. After using the present invention, the rising edge and the falling edge correspond to the same distance and deviation output with the same control amount, which avoids the occurrence of the above situation, makes it easier to obtain the real shape, and has a positive protective effect on the sample and the instrument at the same time.
3、本发明可以使成像系统分辨处宽度更小的凹坑特征。对于宽度较小的凹坑形貌,由于在下降沿跟踪速度较慢,探针还没跟踪到凹坑的深度就已经扫过了它的宽度区域,使得在图像中显示为一个比实际深度更浅的凹坑甚至显示为平面。本发明加快了探针对下降沿的响应速度,因此对于这类形貌有更准确的成像能力。3. The present invention enables the imaging system to distinguish pit features with a smaller width. For the pit shape with small width, due to the slow tracking speed on the falling edge, the probe has swept through its width area before tracking the depth of the pit, which makes it appear in the image as a deeper depth than the actual depth. Shallow pits even appear flat. The invention speeds up the response speed of the probe to the falling edge, so it has more accurate imaging capability for this type of shape.
附图说明Description of drawings
图1为本发明SICM探针与样品间距离自适应控制方法的流程图;Fig. 1 is the flowchart of the distance self-adaptive control method between SICM probe and sample of the present invention;
图2为本发明闭环系统控制框图;Fig. 2 is a closed-loop system control block diagram of the present invention;
图3a为本发明探针逼近样品过程中的电流幅值变化曲线图,即逼近曲线图;Fig. 3 a is the curve diagram of the current amplitude change during the process of the probe approaching the sample of the present invention, that is, the approximation curve diagram;
图3b为本发明探针逼近样品过程的电流偏差幅值曲线图;Fig. 3b is a curve diagram of the current deviation amplitude during the process of the probe approaching the sample of the present invention;
图3c为本发明下降沿补偿函数模型曲线图;Fig. 3c is a curve diagram of the falling edge compensation function model of the present invention;
图4为本发明具体实施方式中步骤3的流程图;Fig. 4 is the flowchart of step 3 in the specific embodiment of the present invention;
图5为本发明方法与普通PID控制方法对高度阶跃的响应特性曲线对比图;Fig. 5 is the contrast diagram of the response characteristic curve of the method of the present invention and common PID control method to height step;
图6a为使用普通PID控制系统的成像结果;Figure 6a is the imaging result using a common PID control system;
图6b为使用自适应距离控制系统下的成像结果;Figure 6b is the imaging result using the adaptive distance control system;
图6c为两个成像结果的截面曲线图。Figure 6c is a cross-sectional graph of two imaging results.
具体实施方式Detailed ways
下面结合附图对本发明做进一步详述。The present invention will be described in further detail below in conjunction with the accompanying drawings.
一种SICM的探针与样品间距离自适应控制方法,包括:A method for adaptively controlling the distance between a SICM probe and a sample, comprising:
步骤1、在开始扫描前做逼近曲线,该逼近曲线为探针/样品距离与离子电流的关系曲线,利用逼近曲线建立下降沿补偿函数模型,该模型以探针当前位置与工作点位置的Z轴压电陶瓷电压差值为输入,以对应相同距离的上升沿和下降沿电流偏差的比为输出;Step 1. Make an approximation curve before starting scanning. The approximation curve is the relationship curve between the probe/sample distance and the ion current. Use the approximation curve to establish a falling edge compensation function model. The model uses the Z of the current position of the probe and the position of the working point The voltage difference of the axial piezoelectric ceramic is the input, and the output is the ratio of the current deviation between the rising edge and the falling edge corresponding to the same distance;
步骤2、扫描过程中记录图像上一行的扫描高度,作为当前待扫描行的预测高度;Step 2. During the scanning process, record the scanning height of the previous line of the image as the predicted height of the current line to be scanned;
步骤3、扫描当前行时,采集压电陶瓷的实时位置,将探针当前位置与预测的工作点位置的Z轴压电陶瓷电压差值作为参数代入下降沿补偿函数模型,得到下降沿补偿系数;Step 3. When scanning the current row, collect the real-time position of the piezoelectric ceramic, and substitute the Z-axis piezoelectric ceramic voltage difference between the current position of the probe and the predicted working point position as a parameter into the falling edge compensation function model to obtain the falling edge compensation coefficient ;
步骤4、判断当前位置是否为高度下降沿,若是则将反馈电流偏差乘以下降沿补偿系数作为反馈回路中新的偏差输送给控制器;Step 4. Determine whether the current position is a falling edge of altitude, and if so, multiply the feedback current deviation by the falling edge compensation coefficient as a new deviation in the feedback loop and send it to the controller;
步骤5、控制器输出控制量给执行机构压电陶瓷,使探针跟踪样品的形貌高度,与样品表面保持恒定的距离。Step 5. The controller outputs the control amount to the actuator piezoelectric ceramics, so that the probe tracks the shape height of the sample and maintains a constant distance from the sample surface.
所述步骤1包括:Said step 1 includes:
步骤1-1、获得探针/样品距离与电流关系的全貌逼近曲线,该曲线反应了离子电流从最大值减小到接近为零的全部过程;Step 1-1. Obtain the overall approximation curve of the relationship between the probe/sample distance and the current, which reflects the entire process of ion current reduction from the maximum value to close to zero;
步骤1-2、利用逼近曲线通过拟合的方式建立下降沿补偿函数模型,该函数的输出为下降沿的电流偏差需要增加的倍数。Step 1-2, using the approximation curve to establish a falling edge compensation function model by means of fitting, and the output of this function is the multiple that the current deviation of the falling edge needs to increase.
所述步骤1-2包括:The steps 1-2 include:
步骤1-2-1、以图像扫描时的电流设定值(95%-99%)为中间点将逼近曲线分成左右即高度上升和高度下降两部分;Step 1-2-1, taking the current setting value (95%-99%) during image scanning as the middle point to divide the approximation curve into two parts, the left and right, that is, the height rise and the height fall;
步骤1-2-2、在高度上升和高度下降两部分中,以离子电流与电流设定值之间的电流偏差的绝对值为函数值,以Z轴压电陶瓷电压与电流设定值处所对应的Z轴压电陶瓷电压之差的绝对值为自变量,分别做出上升沿和下降沿的电流偏差随Z轴压电陶瓷电压差值的变化曲线;Step 1-2-2. In the two parts of height rise and height fall, the absolute value of the current deviation between the ion current and the current setting value is used as the function value, and the Z-axis piezoelectric ceramic voltage and current setting value are used. The absolute value of the corresponding Z-axis piezoelectric ceramic voltage difference is an independent variable, and the variation curves of the current deviation of the rising edge and the falling edge with the Z-axis piezoelectric ceramic voltage difference are drawn respectively;
步骤1-2-3、以正偏差与负偏差绝对值的比作为函数值,以探针当前位置与工作点位置的Z轴压电陶瓷电压差值为自变量,采用最小二乘法进行有理数拟合得到系数,建立下降沿补偿函数模型。Step 1-2-3, using the ratio of the absolute value of the positive deviation to the negative deviation as the function value, taking the Z-axis piezoelectric ceramic voltage difference between the current position of the probe and the working point as the independent variable, and using the least square method to simulate Combined to get the coefficients, and establish the falling edge compensation function model.
所述步骤3包括:Said step 3 includes:
步骤3-1、实时采集压电陶瓷的电压代表探针的当前位置;Step 3-1, collecting the voltage of the piezoelectric ceramic in real time to represent the current position of the probe;
步骤3-2、将探针当前位置与该点预测高度位置的压电陶瓷电压相减,得到代表当前位置与预测工作点位置距离的电压差值;Step 3-2, subtracting the current position of the probe from the piezoelectric ceramic voltage at the predicted height position of the point to obtain a voltage difference representing the distance between the current position and the predicted working point position;
步骤3-3、将探针当前位置与预测工作点位置的电压差值作为自变量代入下降沿补偿函数模型,得到下降沿补偿系数K。Step 3-3. Substitute the voltage difference between the current position of the probe and the predicted working point as an independent variable into the falling edge compensation function model to obtain the falling edge compensation coefficient K.
所述步骤4包括:Said step 4 includes:
步骤4-1、实时采集离子电流及压电陶瓷电压;Step 4-1, collecting ion current and piezoelectric ceramic voltage in real time;
步骤4-2、判断当前扫描点是样品高度的上升沿还是下降沿;Step 4-2, judging whether the current scanning point is the rising edge or the falling edge of the sample height;
步骤4-3、如果是上升沿则电流偏差保持原来的值不变,如果是下降沿则更新电流偏差为原电流偏差乘以下降沿补偿系数K。Step 4-3: If it is a rising edge, the current deviation remains unchanged; if it is a falling edge, update the current deviation to be the original current deviation multiplied by the falling edge compensation coefficient K.
所述步骤4-2包括:Said step 4-2 comprises:
步骤4-2-1、设定一个离子电流偏差值和一个压电陶瓷的电压差值作为电流死区和电压死区;Step 4-2-1, setting an ion current deviation value and a piezoelectric ceramic voltage difference as the current dead zone and the voltage dead zone;
步骤4-2-2、当电流偏差和电压差值分别超出电流死区和电压死区时,判断为样品高度的下降沿,否则为高度上升沿。Step 4-2-2. When the current deviation and the voltage difference exceed the current dead zone and the voltage dead zone respectively, it is judged as the falling edge of the sample height, otherwise it is judged as the rising edge of the height.
一种SICM的探针与样品间距离自适应控制系统,包括:A SICM self-adaptive control system for the distance between a probe and a sample, comprising:
逼近曲线模块:设定探针逼近停止点,获得逼近曲线数据;Approach curve module: set the probe approach stop point, and obtain the approach curve data;
下降沿补偿函数模型建立模块:设定扫描工作点,以工作点为中点通过逼近曲线绘制电流偏差随探针到工作点位置的距离变化的曲线,拟合得到正负偏差比值和反映探针当前位置到工作点位置距离的Z轴压电陶瓷电压差值的关系曲线,建立下降沿补偿函数模型;Falling edge compensation function model building module: set the scanning working point, use the working point as the midpoint to draw the curve of the current deviation with the distance from the probe to the working point through the approximation curve, and get the positive and negative deviation ratio and reflect the probe The relationship curve of the Z-axis piezoelectric ceramic voltage difference between the current position and the working point position, and the establishment of the falling edge compensation function model;
行预测模块:保存当前行每一点的高度信息,在对下一行扫描时提供给控制模块作为高度的预测值;Row prediction module: save the height information of each point in the current row, and provide it to the control module as the predicted value of height when scanning the next row;
反馈控制模块:用下降沿补偿函数模型处理电流偏差得到新的偏差,将新的偏差输入到PID控制器得到控制量,输出控制量到压电陶瓷控制探针的高度以跟踪样品表面的形貌。Feedback control module: Use the falling edge compensation function model to process the current deviation to obtain a new deviation, input the new deviation to the PID controller to obtain the control value, and output the control value to the piezoelectric ceramic to control the height of the probe to track the shape of the sample surface .
本发明为一种SICM探针与样品间距离的新的控制方法,如图1:通过逼近曲线建立下降沿补偿函数模型,结合行预测的方法,实时更新下降沿补偿系数,进而将下降沿处的电流偏差增加到与上升沿同样的水平,消除逼近曲线非线性对下降沿成像的影响。图2为本系统的控制回路框图。The present invention is a new control method for the distance between the SICM probe and the sample, as shown in Figure 1: the falling edge compensation function model is established through the approximation curve, combined with the line prediction method, the falling edge compensation coefficient is updated in real time, and then the falling edge position The current deviation is increased to the same level as the rising edge, eliminating the effect of the nonlinearity of the approximation curve on the imaging of the falling edge. Figure 2 is a block diagram of the control loop of the system.
所述一种SICM探针样品间距离的自适应控制方法包括以下步骤:The self-adaptive control method of the distance between described a kind of SICM probe sample comprises the following steps:
步骤1、在开始扫描前做逼近曲线,该逼近曲线为探针/样品距离与离子电流的关系曲线,利用逼近曲线建立下降沿补偿函数模型,该模型以探针当前位置与工作点位置的压电陶瓷电压差值为输入,以对应的上升沿和下降沿电流偏差的比为输出;Step 1. Make an approximation curve before starting scanning. The approximation curve is the relationship curve between the probe/sample distance and the ion current. Use the approximation curve to establish a falling edge compensation function model. The model uses the pressure between the current position of the probe and the working point position The voltage difference of the electroceramic is input, and the ratio of the corresponding rising edge and falling edge current deviation is the output;
所述步骤1包括:Said step 1 includes:
步骤1-1、如图3a所示,获得探针/样品距离与电流关系的全貌逼近曲线,设置探针逼近的停止条件为离子电流达到最大电流的10%-30%,该曲线反应了离子电流从最大值减小到接近为零的全部过程;Step 1-1, as shown in Figure 3a, obtain the overall approximation curve of the relationship between the probe/sample distance and the current, set the stop condition of the probe approximation as the ion current reaches 10%-30% of the maximum current, and the curve reflects the ion The whole process of the current decreasing from the maximum value to close to zero;
步骤1-2、利用逼近曲线通过拟合的方式建立下降沿补偿函数模型,该模型的输出为下降沿的电流偏差需要增加的倍数。Step 1-2, using the approximation curve to establish a falling edge compensation function model by means of fitting, and the output of the model is the multiple that the current deviation of the falling edge needs to increase.
所述步骤1-2包括:The steps 1-2 include:
步骤1-2-1、以图像扫描时的要使用的电流设定值为中间点即分界点,设定值通常为探针与样品表面距离较远(电流恒定且最大)时电流的95%-99%,将逼近曲线分成左右两部分,左边代表样品高度下降沿的情况,右边代表样品高度上升沿的情况;Step 1-2-1. Use the current set value to be used during image scanning as the middle point, which is the cut-off point. The set value is usually 95% of the current when the distance between the probe and the sample surface is relatively long (the current is constant and maximum). -99%, divide the approximation curve into left and right parts, the left side represents the situation of the falling edge of the sample height, and the right side represents the situation of the rising edge of the sample height;
步骤1-2-2、如图3b所示,以离子电流与电流设定值之间的电流偏差的绝对值为函数值,以Z轴压电陶瓷电压与电流设定值处所对应的Z轴压电陶瓷电压之差的绝对值为自变量,用来表示探针当前位置到工作点位置的距离,分别做出上升沿和下降沿的电流偏差随Z轴压电陶瓷电压差值的变化曲线,代表了探针位于样品的上升沿和下降沿时的电流偏差与压电陶瓷电压差值的关系;Step 1-2-2, as shown in Figure 3b, take the absolute value of the current deviation between the ion current and the current setting value as the function value, and use the Z-axis corresponding to the Z-axis piezoelectric ceramic voltage and current setting value The absolute value of the piezoelectric ceramic voltage difference is an independent variable, which is used to represent the distance from the current position of the probe to the working point, and the variation curves of the current deviation of the rising edge and the falling edge with the Z-axis piezoelectric ceramic voltage difference are drawn respectively. , represents the relationship between the current deviation and the piezoelectric ceramic voltage difference when the probe is on the rising and falling edges of the sample;
步骤1-2-3、如图3c所示,以正偏差与负偏差绝对值的比作为函数值,以反映探针当前位置到工作点位置距离的Z轴压电陶瓷电压差值为自变量,采用最小二乘法进行有理数拟合得到系数,建立下降沿补偿函数:Step 1-2-3, as shown in Figure 3c, use the ratio of the absolute value of the positive deviation to the negative deviation as the function value, and use the Z-axis piezoelectric ceramic voltage difference reflecting the distance from the current position of the probe to the working point as the independent variable , use the least squares method to fit rational numbers to get the coefficients, and establish the falling edge compensation function:
k(d)=(p1×d+p2)/(d+q1) (1)k(d)=(p1×d+p2)/(d+q1) (1)
其中k(d)为下降沿补偿系数,d为反映探针当前位置与工作点位置距离的Z轴压电陶瓷电压差值,p1,p2,q1为系数,通过逼近曲线由有理数拟合得到。Among them, k(d) is the falling edge compensation coefficient, d is the Z-axis piezoelectric ceramic voltage difference reflecting the distance between the current position of the probe and the working point, and p1, p2, q1 are coefficients, which are obtained by fitting rational numbers through the approximation curve.
步骤2、扫描过程中记录代表图像上一像素行扫描高度的压电陶瓷电压,作为当前待扫描像素行高度的预测,Step 2. During the scanning process, record the piezoelectric ceramic voltage representing the scan height of a pixel row on the image as a prediction of the row height of the pixel to be scanned currently.
hp(x,y)=h(x,y-1) (2)h p (x,y)=h(x,y-1) (2)
其中(x,y)表示为图像中的第x行、第y列的像素点,hp为预测高度,h为扫描高度;Where (x, y) is represented as the pixel point of row x and column y in the image, h p is the predicted height, and h is the scanning height;
步骤3、扫描当前行时,采集压电陶瓷的实时位置,将预测目标位置和当前实时位置处的压电陶瓷电压差值作为参数代入下降沿补偿函数模型,得到下降沿补偿系数,如图4。如果当前扫描行为图像的第一行,则仅使用普通PID控制方法进行扫描,不进行行预测的过程;Step 3. When scanning the current line, collect the real-time position of the piezoelectric ceramic, and substitute the voltage difference between the predicted target position and the current real-time position of the piezoelectric ceramic as a parameter into the falling edge compensation function model to obtain the falling edge compensation coefficient, as shown in Figure 4 . If the current scanning behavior is the first line of the image, only the ordinary PID control method is used for scanning, and the process of line prediction is not performed;
所述步骤3包括:Said step 3 includes:
步骤3-1、实时采集压电陶瓷的电压代表探针的当前位置hz_piezo;Step 3-1, collecting the voltage of the piezoelectric ceramic in real time represents the current position h z_piezo of the probe;
步骤3-2、将当前位置的高度与该点预测高度相减,得到当前位置与工作点位置的距离d,用Z轴压电陶瓷的电压差值来表示:Step 3-2. Subtract the height of the current position from the predicted height of the point to obtain the distance d between the current position and the position of the working point, expressed by the voltage difference of the Z-axis piezoelectric ceramic:
d(t)=hz_piezo(t)-hp(x,y) (3)d(t)=h z_piezo (t)-h p (x,y) (3)
步骤3-3、将当前位置与工作点位置的距离作为自变量代入下降沿补偿函数模型,得到下降沿补偿系数k。Step 3-3. Substituting the distance between the current position and the working point as an independent variable into the falling edge compensation function model to obtain the falling edge compensation coefficient k.
步骤4、判断当前位置是否为高度下降沿,若是则将反馈电流偏差乘以下降沿补偿系数作为反馈回路中新的偏差输送给控制器;Step 4. Determine whether the current position is a falling edge of altitude, and if so, multiply the feedback current deviation by the falling edge compensation coefficient as a new deviation in the feedback loop and send it to the controller;
所述步骤4包括:Said step 4 includes:
步骤4-1、实时采集离子电流及压电陶瓷电压;Step 4-1, collecting ion current and piezoelectric ceramic voltage in real time;
步骤4-2、判断当前扫描点是样品高度的上升沿还是下降沿;Step 4-2, judging whether the current scanning point is the rising edge or the falling edge of the sample height;
所述步骤4-2包括:Said step 4-2 comprises:
步骤4-2-1、为避免噪声的影响及两行之间高度突变的影响,设置一个电流死区ideadzone,为避免压电陶瓷振动的影响设置一个压电陶瓷距离死区ddeadzone;Step 4-2-1. In order to avoid the influence of noise and the influence of height mutation between two rows, a current dead zone i deadzone is set, and a piezoelectric ceramic distance dead zone d deadzone is set to avoid the influence of piezoelectric ceramic vibration;
步骤4-2-2、下降沿判定条件:Step 4-2-2, Falling edge judgment condition:
步骤4-3、如果是上升沿则电流偏差保持原来的值不变,如果是下降沿则更新电流偏差为原电流偏差乘以下降沿补偿系数k。Step 4-3. If it is a rising edge, the current deviation keeps the original value unchanged; if it is a falling edge, update the current deviation to be the original current deviation multiplied by the falling edge compensation coefficient k.
e(t)=k(d(t))×(i(t)-isp) (5)e(t)=k(d(t))×(i(t)-i sp ) (5)
其中,upward和downward分别表示上升沿和下降沿,e(t)表示新的电流偏差,i(t)表示反馈量即离子电流,isp表示电流设定值。Among them, upward and downward respectively represent the rising edge and falling edge, e(t) represents the new current deviation, i(t) represents the feedback amount, that is, the ion current, and i sp represents the current setting value.
步骤5、控制器输出控制量给执行机构压电陶瓷,使探针跟踪样品的形貌高度,与样品表面保持恒定的距离。Step 5. The controller outputs the control amount to the actuator piezoelectric ceramics, so that the probe tracks the shape height of the sample and maintains a constant distance from the sample surface.
为验证本发明在使用SICM系统成像时对探针样品间距离的控制性能,进行了对高度阶跃的响应特性实验及对标准PDMS栅格样品的成像实验。在扫描过程中手动给予样品一个向下的高度阶跃,分别采用上述自适应控制方法和普通PID控制方法,记录探针跟踪高度变化的过程,记录响应特性曲线。使用纳米平台令样品产生一个1微米的下降沿,如图5,分别使用普通PID和自适应控制让探针对其进行跟踪,两种情形采用的PID参数相同,普通PID控制方法探针跟踪的轨迹为右边斜率较小的曲线,完成跟踪的时间大于100ms,使用自适应控制方法探针跟踪的轨迹为左边斜率较大的曲线,完成跟踪的时间小于10ms,因而采用SICM探针样品间距离的自适应控制方法使得探针对下降沿的跟踪速度更快,明显优于普通PID控制方法。In order to verify the control performance of the present invention on the distance between probes and samples when using SICM system imaging, the response characteristic experiment to the height step and the imaging experiment on the standard PDMS grid sample were carried out. During the scanning process, the sample is manually given a downward height step, and the above-mentioned adaptive control method and ordinary PID control method are used respectively to record the process of the probe tracking the height change and record the response characteristic curve. Use the nanometer platform to make the sample produce a 1 micron falling edge, as shown in Figure 5, use ordinary PID and adaptive control to let the probe track it, the PID parameters used in the two cases are the same, the ordinary PID control method probe tracking The trajectory is a curve with a small slope on the right, and the time to complete the tracking is greater than 100ms. The trajectory tracked by the probe using the adaptive control method is a curve with a large slope on the left, and the time to complete the tracking is less than 10ms. Therefore, the distance between the samples of the SICM probe is used The adaptive control method makes the probe track the falling edge faster, which is obviously better than the ordinary PID control method.
图6a-图6c为本发明控制系统下对栅格的扫描结果与普通PID控制系统下的扫描结果比较图;图6a-图6b分别采用普通PID和自适应控制对栅格样品扫描,两者采用的PID参数均相同。扫描用的栅格样品每个栅格宽5μm,深200nm,材料选用聚二甲基硅氧烷(PDMS)。使用普通PID控制扫描出的图像在左边栅格上升沿处清晰,但在右边下降沿处比较模糊,如图6a;使用自适应控制扫描出的图像在左边栅格上升沿处的成像效果与使用PID控制时一致,但在右边下降沿处更加清晰,消除了拖尾的现象,如图6b。在同一位置对两幅图像做切面图,显示出本发明的方法使得栅格下降沿处的高度曲线与原方法相比更加陡峭,更接近于真实的形貌,如图6c,验证了其控制性能的优势。Fig. 6a-Fig. 6c is the scanning result of the grid under the control system of the present invention and the scanning result comparison diagram under the common PID control system; Fig. 6a-Fig. The PID parameters used are the same. The grid sample used for scanning is 5 μm wide and 200 nm deep, and the material is polydimethylsiloxane (PDMS). The image scanned using ordinary PID control is clear at the rising edge of the left grid, but blurred at the falling edge of the right, as shown in Figure 6a; the imaging effect of the image scanned using adaptive control at the rising edge of the left grid is the same as that The PID control is consistent, but it is clearer at the falling edge on the right, eliminating the tailing phenomenon, as shown in Figure 6b. Cutting the two images at the same position, it shows that the method of the present invention makes the height curve at the falling edge of the grid steeper than the original method, and is closer to the real shape, as shown in Figure 6c, which verifies its control performance advantage.
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